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通过对提取方法和色谱、质谱条件的改进,建立了纺织品中N-甲基吡咯烷酮(NMP)的气相色谱-质谱联用测定法。纺织材料试样经乙酸乙酯超声波提取,提取液浓缩后用滤纸过滤净化,采用气相色谱-质谱仪(GC-MSD)测定,外标法定量,选择离子监测进行阳性确证。结果表明,当添加N-甲基吡咯烷酮浓度为1μg/mL~10μg/mL时,待测纺织品试样中N-甲基吡咯烷酮的回收率达95.8%,相对标准偏差RSD(n=7)小于5%,其最低检出限为0.05μg/mL,本方法操作简单、快速、准确,灵敏度高,重现性好,可用于纺织品中N-甲基吡咯烷酮的日常检测。
Through the extraction method and the improvement of chromatographic and mass spectrometric conditions, a gas chromatography-mass spectrometry method for the determination of N-methyl pyrrolidone (NMP) in textiles was established. Samples of textile materials were extracted with ethyl acetate. The extracts were concentrated and purified by filter paper. The samples were determined by gas chromatography-mass spectrometry (GC-MSD) and external standard method. The results showed that the recovery of N-methylpyrrolidone was 95.8% when the concentration of N-methyl pyrrolidone was 1μg / mL ~ 10μg / mL, the relative standard deviation RSD (n = 7) was less than 5 %, The detection limit of which is 0.05μg / mL. The method is simple, rapid, accurate, sensitive and reproducible. It can be used in routine testing of N-methylpyrrolidone in textiles.